Development and experimental evaluation of hybrid K-edge/X-ray fluorescence densitometer for uranium solution measurement

Abstract

The hybrid K-edge/X-ray fluorescence densitometer (HKED) is a combination of K-edge absorption technology (KED) and characteristic X-ray fluorescence (XRF), which has the advantages of direct, fast and non-destructive determination, and is an ideal non-destructive measurement technology for uranium and plutonium concentrations. In this paper, a new HKED was developed, primarily utilizing an X-ray tube from COMET, alongside high-purity germanium (HPGe) and cadmium telluride (CdTe) detectors from AMETEK ORTEC. This manuscript delves into several variables that influence measurement outcomes under predefined experimental conditions and operational prerequisites to pinpoint critical parameters. It was discerned that the adoption of a 160 kV high voltage setting markedly diminishes experimental interferences, while the beam current, optimally set at 2 mA, not only ensures a linear correlation with the count rate but also maximizes the effective count detected. The incorporation of a 2 cm fixed-length iron rod along the trajectory between the sample and the detector, complemented by an additional 3 mm external absorber before the KED detector, effectively mitigates direct X-ray exposure, thereby enhancing transmittance values to attainable extents. Subsequent to the determination of these pivotal parameters, validation of the HKED system's efficacy was conducted via performance evaluation tests on a laboratory-scale HKED setup. Measurements undertaken for both KED and XRF across an interval ranging from 300 to 3000 s fell within the 2σ boundary, affirming the system's stability. Repeated measurements of 50 g/L and 150 g/L uranium solutions yielded KED precision rates of 0.56% and 0.19%, respectively. Moreover, linear regression analyses linking transmittance, characteristic X-ray fluorescence, and uranium concentrations across a spectrum of 0–150 g/L underscored the laboratory HKED instrument's robust analytical capabilities. Notably, the relative discrepancy between theoretical predictions and empirical findings for the 150 g/L uranium sample was minimized to a commendable 0.58%.